81results about How to "Reasonable reaction process design" patented technology

The invention discloses a preparation method of 7-O-ethyl morroniside. The best preparation process of 7-O-ethyl morroniside was screened out through a large number of experiments, including dissolution method, reaction pH value, heating temperature, heating time and other parameters, and the best purification method was optimized, and the entire reaction process design Reasonable, strong operability, high synthesis rate of 7‑O‑ethyl morroniside, less impurities, high purity, low cost, and industrial production can be realized. The present invention is further screened through in vivo and in vitro anti-inflammatory experiments, and the results show that 7-O-ethyl morroniside has good anti-inflammatory effects both in vivo and in vitro, and has the potential use of being prepared as an anti-inflammatory drug.

The invention discloses a method for preparing tiotropium bromide, which comprises the following steps of: preparing scopine-2,2-dithienyl glycolate from scopine and methyl 2,2-dithienyl glycolate, reacting the scopine-2,2-dithienyl glycolate with methyl bromide to prepare a tiotropium bromide crude product, and refining the tiotropium bromide crude product to obtain a tiotropium bromide finishedproduct. The method is characterized in that: the scopine and the methyl 2,2-dithienyl glycolate undergo ester exchange reaction under the action of dimethylbenzene, and the mixed catalysts of sodiumand sodium methoxide, and after the reaction, reaction solution is post-treated to obtain the scopine-2,2-dithienyl glycolate. In the method, in the process of preparing the scopine-2,2-dithienyl glycolate, the sodium and the sodium methoxide are simultaneously taken as the catalysts, and scopine isomer content after the reaction is less than 0.1 percent which completely meets specifications in the trial standards of European pharmacopoeia; and the method solves a big problem for the conventional preparation of the tiotropium bromide and is easy to realize industrial production.

The invention relates to a preparation method of 2-((1S3aR7aR)-5-tert-butyloxycarbonyltetrahydrofuro[3,4]piperidine-1)acetic acid. The preparation method comprises 11 steps: carrying out esterification on a dicarboxylic acid piperidine compound 1 in thionyl chloride to obtain a diester compound 2; then reducing a pyridine ring by utilizing palladium carbon to obtain a compound 3; then taking the compound 3 to react with Boc acid anhydride to obtain a Boc protected compound 4; hydrolyzing the compound 4 by utilizing lithium hydroxide to obtain a dicarboxylic acid compound 5; carrying out ring closure in acetic anhydride to obtain a compound 6; carrying out reduction and ring opening by utilizing NaBH4 to obtain a mixture of position isomerism compounds 7A and 7B; carrying out the ring closure in the presence of iodomethane and potassium carbonate to generate position isomerism lactone 8A and 8B; step 8, reducing the 8A, obtained by column passing separation, by utilizing DIBAH (Diisobutylaluminum Hydride) to obtain a compound 9; carrying out Wittig reaction to obtain a compound 10; carrying out Michael addition under an alkaline condition to obtain a compound 11; finally, hydrolyzing the compound 11 under the alkaline condition to obtain a final compound.

The invention relates to a method for preparing tert-butyl-1,8-dioxa-4,11-diazaspiro[5.6]dodecane-11-carboxylate, which mainly solves the problem that there is currently no technology suitable for industrial synthesis methods question. The present invention is divided into six steps: the first step, first dissolving compound 1 in dichloromethane, then adding Boc anhydride, and reacting to obtain compound 2; the second step, compound 2 and sodium hydrogen, 3-chloro-2-chloromethyl ‑1‑propylene reaction to obtain compound 3; in the third step, compound 3 is dissolved in dichloromethane, and m-chloroperoxybenzoic acid is added to react to obtain compound 4; in the fourth step, compound 4 is reacted in 2‑benzylaminoethanol Compound 5 was obtained; in the fifth step, compound 5 was reacted with sodium hydrogen and p-toluenesulfonimidazole in tetrahydrofuran to obtain compound 6; in the sixth step, compound 6 was reacted with palladium hydroxide in methanol to obtain final compound 7.